Laboratory distillation testing apparatus



July 14, 1959 c. M. woLsToN; JR; ET AL 2,894,881

A LABORATORY DISTILLATION TESTING APPARATUS Filed Nov. 29, 1955 2 Shets-Sheet 1 \i w w '7 7 July 14, I c. M. WOLSTON, JR., ET AL- 2, 4

LABORATORY DISTILLATION TESTING APPARATUS Filed Nov. 29, 1955 2 Sheets-Sheet 2 GEORGE W JZc/c United States Patent LABORATORY DISTILLAT'ION DESTING APPARATUS Clinton M. Wolston, Jr., and George W. Jack, Di n, Tex., assignors to The American Oil Company, Texas City, Tex., a corporation of Texas a Application November 29, 1955, Serial No. 549,640 9 Claims. (Cl. 202-172) This invention relates to an apparatus for testing petroleum products and particularly relates to improvements in distillation apparatus adapted for use in inspection laboratories.

The distillation apparatus of the type to which this invention relates includes a condenser box, a condenser tube which extends within the condenser box and is connected to a distillation flask, a distillation shield supporting the flask and a heating unit therefor, and a receiver into which the condenser tube discharges.

Heretofore, various types and designs of such distillation equipment have been proposed but the prior devices have not been entirely satisfactory from one or more standpoints.

It is a primary object of our invention to provide an improved distillation testing apparatus which is compact in form, can be readily assembled in a variety of multiple unit installations, and is so arranged that when assembled as multiple units the operator can view from one end of the unit all the receivers. A further object of the invention is to provide a readily demountable panelunit which may be interchanged with other units. Still another object of the invention is to provide illumination means behind each receiver which permits more accurate and rapid reading of the graduated receivers.

An additional object of ourinvention is to provide means for rapid cooling of the distillation flask at the completion of the heating cycle. Another object of our invention is to provide an apparatus wherein the front panels of the distillation shields and the exposed wall portions of the condenser box present a continuous front wall; 7 These and other objects of our invention will become "apparent as the description thereof proceeds.

In practice, a predetermined quantity of the sample is poured into the distillation flask. The condenser box contains cooling water maintained at the desired temperature bycooli'n'g coils and, if desired, a suitable circulator. =A graduated receiver is arranged in front of the cabinet below the outlet end ofthe condenser tube, one such receiverbein'g used in-conjunction with each flask and" each condenser tube. -Heat-is applied at a uniform rate to the flask and condensate is discharged from the condenser tube associated with the flask into the respective receiver. When the first drop falls from the end of the condenser tube into thedesignated receiver, the reading of the flask thermometer is recorded as the initial boiling point.

The heat applied to the flask is then so regulated that the distillation proceeds at a uniform rate, the reading of thetdistillation thermometer being taken when 10 cc. of distillatefhas been collected in the graduated receiver. The. heating is continued until the temperature level reaches a maximum and begins to drop constantly. This highest temperature observed is recorded as the maximum temperature'andthis pointwill ordinarily bereached after the'b'ottom ofthe flask has become dry. The total volume of di'stillate, collected is recorded as the recovery.

Upon'te- 'ation'of the heating, the flask is rapidly 25 secured by wing nuts 26 cooled and any vapors therein are condensed and poured from the flask into a small graduated cylinder for a determination of the total volume of liquid residue. The difference between the initial volume of the liquid sample and the sum of the recovery and the residue is calculated and recorded as distillate loss.

To illustrate our invention, it will be described with reference to an embodiment which is adapted foruse in making petroleum distillation tests in accordance with the standards of the ASTM, such embodiment being shown in the accompanying drawings wherein:

Figure l is a front elevation of the apparatus;

Figure 2 is a plan view, partly in section, of the apparatus in Figure l;

Figure 3 is a side elevation, partly in section;

Figure 4 is a top view of Figure 3; and

Figure 5 is a fragmentary diagram of an embodiment of the invention.

Referring to the drawings, the apparatus illustrated comprises a multi-unit apparatus in which provision is made for simultaneously conducting independent distillation tests on several liquid samples. The apparatus includes a generally rectangular condenser box or cabinet 10 which may be provided with a suitable cover 10a. The box 10 has a metal liner 11 (Figure 2) and a suitable thermal insulation 12 such as cork. The outer walls of the box 10 are extended below the bottom 10b of the box 10 to provide a stand for the box. The exposed wall 13 of the cabinet 10 includes recesses 14 which accom modate the control panels or shields 15.

The shields 15 are removably supported within the' recess 14 which is divided into two compartments by a of a first angular member 22 fixed to a front edge of recess Wall 23 and a nested second angular member 24 providing the grooves 20 and 21.

The panels or shields 15 support an adjustable shelf insulating sheet 27 below heater 28. A powerstat or other heat controller unit 29 having heat control knob 30 exterior of said panel 15 is also fixed to the rear of panel 15. A heater switch 31 controls the power supply from i the powerstat 29. A detachable plug 32 is interposed the heater 28 and the switch 31 and the power supply to the controller or powerstat 29 is a plug-in at the rear base of the cabinet assembly 10 to permit removal of the panel assembly without disturbing any of the permanent electrical connections.

The arrangement of the various elements including the powerstat 29 and heater switch 31 and the heater 28 on the panel assembly is identical in all of the panels 15 and they are interchangeable with similar panel units in the compartments 14a or 14b of the recesses 14. a

The distillation flask 33 is placed upon the heater 28 within the recess 14 after the tongues 18 and 19 of thepanel assembly have been positioned within the grooves 20 and 21 in the particular compartment. The electrical plugs are connected and the receiver 34 is positioned below the outlet 35 of the condenser tube 36. The condenser tube 36 has its inlet end 37 projecting forwardly of the rear wall 38 of the recess 14 and passes through the condenser box 10 in a smooth curve and forwardly of the exposed wall 39 of the forward bay 10c of the cabinet 10..

Within the condenser box 10 there is provideda cooling fluid and cooling tubes (not shown) together with a circulator (not shown) which may comprise an electrically driven impeller mounted from the hinged top cover 10a of Patented July 1 ,1 59

on which is placed a heat.

the condenser box in a manner which is well known to the art of constant temperature baths.

In the operation of the apparatus described, samples of; liquid to be tested are placed in the flasks 33, which may be viewed through windows 47, and the heater controlknobs 30' on'the shield or panel are adjusted so thaat the required rate of heating is elfected, the heating rate being, indicated by the meters 48-. The vapor from the flasks 33 is discharged into the associated condenser tubes 36 where the vapor is cooled and the distillateproduced discharges into the receivers 34.

.The operator observes the temperature indicated by the thermometers 40 projecting from the flasks 33 as well as the volume of distillate recovered at IO-degree intervals, in. accordance with the ASTM testing procedure. When the maximum temperature has been reached and it begins to fall steadily, this signifies the end of the distillation test. However, it is desired to obtain a product balance which requires the collection and measurement of the vapors within the flask 33 whichare not recovered as distillate in the receivers 34. Accordingly, it is-highly desirable to cool the flasks 33 rapidly under controlled conditions.

We have provided automatic means for cooling the flask 33'at the end of a run which includes an air supply 41', a solenoid-actuated valve 42 and an air discharge duct 43 which passes upwardly through the condenser boxbottom 1% and extends forwardly of the rear wall 38 of: the recess 14to direct a stream of cooling air onto the flask 33'; This solenoid valve 42 can be controlled by the. switch. 49 on theexposed Wall13 of the unit'and,

if desired,v can be connected incircuit with the heater forwardly of the entire unit including'the panels 15 and the exposed wall portions 13 of the condenser box 10. The lower portion of the exposed Wall 13 of the cabinet 10 below the bottom 10]: of the box is provided with a translucent panel 50 which, with lamp 45 mounted at the rear of the cabinet 10, provides a diflused back-lighting for the receivers 34.

With the arrangement of the control panels 15, the

recesses 14 and the narrow condenser b'ox' bays 10c, it

is possible to arrange a maximum number of distillation" units within a given bench'space while providing optimum conditions for the conducting of a large number of ASTM distillations simultaneously by a minimum number of operators. Further, the designof the control panels 15 and the electrical connections thereto make it possible for laboratory technicansto demount a given control panel 15 and replace it with another, should that be desirable.

From the above, it will be apparent that we have attained the objects of our invention and, although it has been described with reference to one embodiment thereof, it should be' understood that this is by way of illustration only and that our invention is not necessarily limited thereto. Furthermore, in view of the description given, modifications in the'construction' andmode of operation'will become apparent to those skilled in the art'and it'is contemplated that such modifications can be rnadewithout departing from the scope of the inventloni What we claim is:

1. Laboratory distillation-testing apparatus having a carried by said shield means for supporting said flask, conduit means below said tank, and solenoid valve means on said conduit means, the discharge end of said conduit means projecting forwardly of the rear wall of said recess below said condenser tube inlet and arranged to discharge forwardly and downwardly towards said shelf means. i a

2. The apparatus or claim 1 whereinsaid recess means accommodates a pair of shields arranged side by side and wherein each of said shields has a flat panel front which is slidably supported in guideslots:

3. In combination with a laboratory test apparatus having a condenser tank, a flask, a flask supporting means, a heating means, a condenser tube passing'through the tank, a light diffusing panel, the improvements which comprise means for supporting said tank in an elevated position, at least one recess in a front wall of said tank, said recess having two side walls and a'rear wall, a shield removably disposed within-said recesss, guide slot meansat the forward edges of saidside walls, a substantially flat panel on the front of said shield having its edges'removably secured within said slots, an adjustable shelf means supported by said panel adapted to hold a distillation flask, and cooling fluid conduit means-discharging into said recess;

4. In alaboratory distillation testing. apparatus including a distillation flask, electrical heater meansfor said flask; a condenser means for the-distillate from said flask,- and a distillate receiver, the improvement which comprises arecess; in the front wall of said con; denser box, said recess having a pair of sidewalls andarear wall, guide slot means on the forward edges of saidside walls; removable flask support arid shield means disposed within said recess, said last-named means having-a vertical panel, the edges of which are slidably secured within said guide slots, an adjustable shelf means supported by the rear face of said panel, a heater means on said shelf, one end of said inclined com denser tube projecting forwardly of the rear wall of said recess in a region above said shelf and the other end of saidcondenser tube projecting-forwardly of a front wall of said condenser box, cooling means comprising a gas conduit projecting forwardly of said rear recess wall below saidcondenser tube inlet and above said heater means, a solenoid valve means on said gas conduit, and

switch means for controlling said heater and said sole-- noid valve means whereby said solenoid valve is open when the heater current is turned ofi.

5. In adistillation testing apparatus the improvement which comprises an'elongated condenser box, a plurality of recesses in the front wall ofsaid box,- said'recesses being adapted to accommodate one or more'flask shields, a cornerrecess at either end of said condenser box each adapted'to receive such a flask shield, at third recess intermittent the end of saidcondenser box adapted to ac-' ditfusion means in the'saidsupporting-wall meansbelow the said condenser tube outlets, each of said flask shields comprising-anupstanding panel, guide slot means at the forward edges of each of 'said' recesses, said 'pan'els being supported withinsaid guide slot means, adjustable" shelves carried by" the rear ofeach'of' said panel's, afias'kheater on eachof' said shelves, a" 'gas=cooling'duct'projectirig forwardly'oreaeh of therarwans of'e'ach of 'said recesses'and downwafdly directing a ct'iolirlg' stream 'of gases into said recesses toward said heaters, cooling coils located within said condenser box, a mummy-memes agitating element suspended from the topof i said con- 5 denser box, a thermometer means projecting downwardly through the top of said condenser box at a point remote from said agitating element, solenoid valve means on said gas cooling ducts, and switch means for controlling said valve means and said heaters, said switch means being mounted on the face of the assembly.

6. In a laboratory distillation testing apparatus the improvement comprising a condenser means embodying a casing, recess means in a wall of said casing, shield means disposed within said recess means, shelf means for supporting a flask in the upper portion of said shield means, means within said shield for applying heat to such flask, an inclined condenser tube disposed within said casing, the inlet of said tube projecting outwardly of a wall of said recess and having its outlet projecting from said casing, a light-difiusing panel in said wall below said outlet, cooling fluid conduit means passing through said casing, and solenoid valve means on said conduit means, the discharge end of said conduit means projecting into said recess and arranged to discharge cooling fluid within said shield.

7. The apparatus of claim 6 wherein said recess means comprises a rectangular three-walled chamber accommodating a pair of shields arranged side by side and .wherein each of said shields has a flat panel front which is slidably supported in guide slots carried by the said wall of the said casing.

8. The improved laboratory distillation testing apparatus comprising a box-like casing, means for supporting said casing in an elevated position, at least one recess in an upstanding wall of said box-like casing, said recess having two side walls and a rear wall, panel means removably disposed between said side walls and across said recess, vertical guide slot means at the forward edges of said side walls supporting said panel, an adjustable shelf means supported on the rear of said panel and adapted to hold a distillation flask within said recess, an electrical heating means associated with said shelf means, an inclined condenser tube loop disposed within said casing, the elevated inlet of said tube projecting forwardly of the rear wall of said recess and the lower outlet of said tube projecting forwardly of a portion of said casing, a light-diifusing panel in said casing wall providing back lighting for a distill-ate receiver disposed below said condenser tube outlet, and valved conduit means discharging a cooling gas into said recess to impinge upon a distillation flask within said recess.

9. The apparatus of claim 1 wherein said heating means comprises an electrical heater, and includes switch means controlling said electrical heater and said solenoid valve whereby said solenoid valve is open when the heater current is 0E and said valve is closed when the heater is on.

References Cited in the file of this patent UNITED STATES PATENTS 440,752 Barotte Nov. 18, 1890 2,222,464 Newman Nov. 19, 1940 2,718,493 Lawler Sept. 20, 1955 

1. LABORATORY DISTILLATION TESTING APPARATUS HAVING A CONDENSER TANK, A FLASK, A FLASK SUPPORTING MEANS, A HEATING MEANS, A CONDENSER TUBE PASSING THROUGH THE SAID TANK, AND A LIGHT DIFFUSING PANEL, THE IMPROVEMENTS WHICH COMPRISE A RECESS IN SAID CONDENSER TANK, A SHIELD MEANS DISPOSED WITHIN SAID RECESS, ADJUSTABLE SHELF MEANS CARRIED BY SAID SHIELD MEANS FOR SUPPORTING SAID FLASK, CONDUIT MEANS BELOW SAID TANK, SOLENOID VALVE MEANS ON SAID CONDUIT MEANS, THE DISCHARGE END OF SAID CONDUIT MEANS PROJECTING FORWARDLY OF THE REAR WALL OF SAID RECESS BELOW SAID CONDENSER TUBE INLET AND ARRANGED TO DISCHARGE FORWARDLY AND DOWNWARDLY TOWARDS SAID SHELF MEANS. 